Fluxing Agents on Ceramification of Composites of MgO-Al_2O_3-SiO_2/Boron Phenolic Resin

Fluxing agents of zinc borate, antimony oxide, galss frit A and glass frit B, with different melting or softening point temperatures, were added into MgO-Al_2O_3-SiO_2/boron phenol formaldehyde resin(MAS/BPF) composites to lower the formation temperature of eutectic liquid phase and promote the ceramification of ceramifiable composites. The effects of fluxing agents on the thermogravimetric properties, phase evolution, and microstructure evolution of MAS/BPF composites were characterized by TG-DSC, XRD and SEM analyses. The results reveal that the addition of a fluxing agent highly reduces the decomposition rate of MAS/BPF composites. Fluxing agents lower the formation temperatures of liquid phases of ceramifiable MAS/BPF composites obviously, and then promote the ceramification and densification process. The final residues of composites are ceramic surrounded by large amount of glass phases.     

Ceramification of Composites of MgO-Al_2O_3-SiO_2/Boron Phenolic Resin with Different Calcine Time

The ceramifiable polymer composite of MgO-Al_2O_3-SiO_2/boron phenolic resin(MAS/BPF) with 40wt% of inorganic fillers was calcined at 1 200 ℃ for different time to promote ceramification of ceramifiable composite and improve heat resistance.The effects of different calcine time on the macroscopical morphology,mass loss,phase evolution,microstructure and chemical bond evolution of MAS/BPF composites were characterized by XRD,XPS,and SEM analyses.The experimental results reveal that the increase of calcine time result in the fewer holes,relatively denser and smoother top layer of MAS/BPF composites and protect the interior from deeper decomposition.The final residues of composites are amorphous carbon and C-O-Si-Al-Mg ceramic.And MAS/BPF composites show excellent mass stability,low shrinkage and self-supporting features after 2 h holding compared with BPF composites without 40wt% of inorganic fillers.     

Investigation on phase evolution of the ZnO-B<Subscript>2</Subscript>O<Subscript>3</Subscript>-SiO<Subscript>2</Subscript> glass ceramics

ZnO-B₂O₃-SiO₂-Al₂O₃-Na₂O glass doped with nucleating agent TiO₂ was prepared with melting-quenching method and the effect of nucleating agent on the crystallization behavior and phase evolution of this glass was investigated by differential thermal analysis (DTA), X-ray diffraction (XRD), and scanning electron microscopy (SEM). The experimental results show that the glass transition temperature and the first crystallization temperature decrease from 630 °C and 765 °C to 595 °C and 740 °C, respectively, with introduction of TiO₂ into glass. There is no diffraction peaks in the XRD pattern but it is no longer transparent for the base glass without nucleating agent after heat treatment, which suggests the serious phase separation occurred, and the observation by SEM indicates that the phase separation is developed by nucleation and growth mechanism. However, there are two different crystals ZnAl₂O₄ and NaAlSiO₄ present in the glass containing TiO₂ after heat treating at 575 °C for 2 h and 740 °C for 6 h, respectively. What is interesting is that NaAlSiO₄ disappears as the crystallization time at 740 °C increases from 6 h to 12 h, and more ZnAl₂O₄ crystal is formed, namely, the further formation of ZnAl₂O₄ is at cost of NaAlSiO₄ with increasing crystallization time. And observation of the morphology of glass ceramics shows great difference with increasing crystallization time. Moreover, the ability of ZnO-B₂O₃-SiO₂-Al₂O₃-Na₂O glass ceramics against attacking of 1M HCl solution is increased by the crystals precipitated in heat treatment process.     

Effect of the Cool System on Internal Stress of CaO-Al203-SiO2 Glass-ceramic System

The samples were attained through altering the cooling system of producing glass-ceramics. The X-ray diffraction was used to test the stress value of different samples. The relation of the cooling system and internal stress were also investigated. The experimental results show that the stress of glass-ceramic had a close relation with starting cool temperature. Above 800 ~C, glass-ceramic could be accelerated cooling and did not bring stress. Temperature between 500 ℃ and 800℃ was an important temperature range of the formation of stress in glass-ceramic, in which the glass-ceramic stress would change obviously. Cool system was the key on how to control and eliminate internal stress in order to reduce the destroy of materials crated by internal stress. In addition, glass particles size increase, glass-ceramic stress increase in consequent.     

Effect of temperature on polishing and flatting time of float-formed Li<Subscript>2</Subscript>O-Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-SiO<Subscript>2</Subscript> glass

Li₂O-Al₂O₃-SiO₂ glass prepared from traditional melting and cooling process was investigated. The surface characteristic of LAS glass was studied by simulating tin bath with different temperature and time, and the effect of surface tension/viscosity ratio on flatting time was analyzed. The results demonstrated that LAS glass can polish effectively when polishing at 1 300 for 8 °C min, and the optimum flatting and polishing temperature was 1 250–1 300 °C.     

Crystallization and luminescence properties of Sm<Superscript>3+</Superscript>-doped SrO-Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-SiO<Subscript>2</Subscript> glass-ceramics

The Sm³⁺-doped SrO-Al₂O₃-SiO₂ (SAS) glass-ceramics with excellent luminescence properties were prepared by batch melting and heat treatment. The crystallization behavior and luminescent properties of the glass-ceramics were investigated by DTA, XRD, SEM and luminescence spectroscopy. The results indicate that the crystal phase precipitated in this system is monocelsian (SrAl₂Si₂O₈) and with the increase of nucleation/crystallization temperature, the crystallite increases from 66 % to 79 %. The Sm³⁺-doped SAS glass-ceramics emit green, orange and red lights centered at 565, 605, 650 and 715 nm under the excitation of 475 nm blue light which can be assigned to the ⁴G_5/2→⁶ H _j/2 (j=5, 7, 9, 11) transitions of Sm³⁺, respectively. Besides, by increasing the crystallization temperature or the concentration of Sm³⁺, the emission lights of the samples located at 565, 605 and 650 nm are intensified significantly. The present results demonstrate that the Sm³⁺-doped SAS glass-ceramics are promising luminescence materials for white LED devices by fine controlling and combining of these three green, orange and red lights in appropriate proportion.     

Effect of ZnO-B<Subscript>2</Subscript>O<Subscript>3</Subscript> glass addition on the microwave dielectric properties of BaO-Nd<Subscript>2</Subscript>O<Subscript>3</Subscript>-TiO<Subscript>2</Subscript>-Bi<Subscript>2</Subscript>O<Subscript>3</Subscript> system

The effect of ZnO-B₂O₃(ZB) glass addition on the sintering behavior, microstructures and microwave dielectric properties of BaO-Nd₂O₃-TiO₂-Bi₂O₃ (BNTB) system was investigated with the aid of X-ray diffraction, scanning electron microscopy and capacitance meter. It is found that the ZB glass addition, acting as a sintering aid, can effectively lower the sintering temperature of BNTB system to 850 °C. The dielectric constant of BNTB-ZB ceramics increases with the increase of soaking time and the value of dielectric loss decreased with increasing soak time. The optical dielectric properties at 1 GHz of ɛ=74, tan δ=4×10⁻⁴, and TCC=25 ppm/°c were obtained for the BNTB system doped with 25 wt% ZB glass sintered at 850 °C for 2 h, representing that the BNTB-ZB ceramics could be promising for multilayer low temperature co-fired ceramics applications.     

Preparation and optical properties of Er<Superscript>3+</Superscript>: Na<Subscript>2</Subscript>O-Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-SiO<Subscript>2</Subscript> transparent glass-ceramics

Na₂O-Al₂O₃-SiO₂ glass-ceramics doped with Er³⁺ ions were synthesized by the conventional melt quenching technique at a low melting temperature. The samples were characterized by differential scanning calorimetry (DSC), X-ray diffraction (XRD), scanning electron microscopy (SEM), UV-vis-NIR scanning spectrophotometry, and fluorescence spectrometry. The results show that the main crystalline phase of glass-ceramics is nepheline.The best heat-treatment process is at 520 °C for 2 h. Because the up-conversion luminescence and near infrared luminescence properties of glass doped with Eu³⁺ are studied in detail.     

Effect of aluminum addition on microstructure and properties of SiO<Subscript>2</Subscript>-B<Subscript>2</Subscript>O<Subscript>3</Subscript>-Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-CaO vitrified bond

Influence of aluminum addition on the structures and properties of SiO₂-B₂O₃-Al₂O₃-CaO vitrified bond at low sintering temperature and high strength was discussed. FTIR and XRD analyses were used to characterize the structures of the basic vitrified bond with different contents of aluminum. The bending strength and the thermal expansion coefficients were also tested. Meanwhile, the microstructures of composite specimens at sintering temperature of 660 °C were observed by scanning electron microscope (SEM). The experimental results showed that the properties of vitrified bond with 1wt% aluminum were improved significantly, where the bending strength, Rockwell hardness, and thermal expansion coefficient of the vitrified bond reached 132 MPa, 63 HRB, and 6.73×10^-6 °C^-1, respectively.     

Glass formation and optical band gap studies on Bi<Subscript>2</Subscript>O<Subscript>3</Subscript>-B<Subscript>2</Subscript>O<Subscript>3</Subscript>-BaO ternary system

The glass forming region of Bi₂O₃-B₂O₃-BaO ternary system was investigated. A serial of glass samples with high Bi₂O₃ content in Bi₂O₃-B₂O₃-BaO system were prepared by using conventional melting and quenching meld, and the refractive indexes and absorption spectra of samples were measured. It is found that the refractive index of samples as well as the UV absorption increase with the increase of BaO content. According to the Tauc law, optical band gap E _opg which is assumed to be the effective energy band gap E _g is calculated and decreases with the increasing BaO content, and the ratio of E _g/E _opg is 1.3.     

Preparation and characteristics of Cu/Al<Subscript>2</Subscript>O<Subscript>3</Subscript>/MgF<Subscript>2</Subscript>/Au tunnel junction

The fabrication process of Cu/Al₂O₃/MgF₂/Au double-barrier metal/insulator/metal junction (DMIMJ) was introduced, and more stable light emission from this junction was successfully observed. The light emission physical mechanism of the junction was discussed. Results show that light emission spectrum of this structure locates at wavelength of 250–700 nm with two peaks at around 460 nm and 640 nm, which moves towards shorter wavelength region in comparison with that of the Al/Al₂O₃/Au junction. The light emission efficiency of this junction ranges from 0.7×10⁻⁵–2.0×10⁻⁵, which is 1 to 2 orders higher than that of the single-barrier Al/Al₂O₃/Au junction. The improved properties of this structure should be due to the electrons resonant tunneling effect in the double-barrier.     

Molten Salt Synthesis of Ba（ Mgl／3Nb2／3 ）O3 Powder

The single-phrase Ba(Mgl/3Nb2/3)O3(BMN) powder was saccessfully prepared by the KCImolten salt synthesis(MSS) method. The temperature for single-phase BMN powders by MSS was about 400℃ lower than that by the solid-phase method. The average particle size (APS) was about 0.91,u.m at 900℃ and increased with increasing synhesis temperature. Based on the APS, the activation energy for particle growth in theMSS, whose value was 64. 1kJmol^-1.was attained. The sinterability of the powder prepared by MSS method wasbetter than that pretared by solid-phase method.     

Synthesis and characterization of a new Fe<Subscript>2</Subscript>O<Subscript>3</Subscript> pillared triple-layered perovskite KSr<Subscript>2</Subscript>Nb<Subscript>3</Subscript>O<Subscript>10</Subscript>

A n-Hexyl NH₃Sr₂Nb₃O₁₀ is obtained by the stepwise ion-exchange reaction, then is dispersed in aqueous solution of trinuclear acetato-hydroxo iron (III) nitrate, [Fe₃(OCOCH₃)₇OH·2H₂O]NO₃, and the interlayer potassium cations of the perovskite niobate are exchanged with the partially hydrolyzed trinuclear acetato complex ions. On heating, the exchanged complex ions are converted into iron oxide pillars which keep the perovskite sheets apart. The product is characterized by XRD, SEM, EDAX and surface area measurement respectively. Zhang Hui: Born in 1970 Funded by the National Natural Science Foundation of China (No. 50002007), Major Program of Ministry of Education (No. 0201) and Open Foundation of State Key Lab of Advanced Tech. for Materials Synthesis and Processing.     

Laser-induced spark ignition of H<Subscript>2</Subscript>/O<Subscript>2</Subscript>/Ar mixtures

Laser-induced spark ignition of hydrogen-oxygen-argon mixtures was experimentally investigated using a Q-swiched Nd:YAG laser to break down the gas at 532 nm. The laser-based high-speed schlieren system was employed to record flame front evolution for the gas mixtures with different initial pressure or laser output energy or argon dilution. The results show that the breakdown of the gas leads to the generation of ellipsoidal plasma. The rarefaction waves create the toroidal rings at the leading and trailing edges of the plasma, which provides a reasonable explanation for inward wrinkle of the plasma and the resultant flame. The toroidal rings at leading edge decays more rapidly and a gas lobe is generated that moves towards the laser. The hot gas in the plasma induces the generation of the spark kernel. Affected by the very weak shock wave or compression waves reflected off the wall, the initial laminar flame decelerates. The arc flame front interactions with the wall, reversed shock wave or compression waves, rarefaction waves, etc. induce the transition from laminar flame to turbulent one. These induce the transition from laminar flame to turbulent flame. For stoichiometric hydrogen-oxygen mixtures diluted by 76.92% argon at an initial pressure of 53.33 kPa, the minimum output energy of the laser is 15 mJ for successful laser-induced spark ignition. With increasing initial pressure or the output energy of the laser, or decreasing argon dilution, the speed of the flame front increases.     

Fabrication and mechanical properties of Al<Subscript>2</Subscript>O<Subscript>3</Subscript>/TiAl composites

Al₂O₃/TiAl composites were successfully fabricated by hot-press-assisted exothermic dispersion method with elemental powder mixtures of Ti, Al TiO₂ and Nb₂O₅, and the microstructure and mechanical properties were investigated. The results indicate the fine Al₂O₃ particles tend to disperse on the grain boundaries. The grain size of TiAl matrix decreases and the hardness increases with increasing Nb₂O₅ content. The bending strength and fracture toughness reach to a maximum when Nb₂O₅ content is 6 wt%, under 642 MPa and 6.69 MPa·m^1/2, respectively. Based on the fractography and the observation of crack propagation path, it is concluded that the strengthening and toughening of such composites at room temperature can be attributed to the refinement of the TiAl matrix, the deflection behavior in the crack propagation and the dispersion of Al₂O₃ particles.     

Progress on RE<Subscript>2</Subscript>O<Subscript>3</Subscript>-Mo/W matrix secondary emitter materials

Two types of secondary emitter materials, the rare earth oxides (RE₂O₃) doped Mo cermet cathodes and the Y₂O₃-W matrix pressed cathode, are introduced in this paper. According to the calculation results, Y₂O₃ exhibits the best secondary emission property among Y₂O₃, La₂O₃, CeO₂ and Lu₂O₃. The rare earth oxides co-doped Mo cathodes in which Y₂O₃ is the main active substance exhibit better secondary emission property than single RE₂O₃ doped Mo cathode. The results obtained by the Monte-Carlo calculation method show that the secondary electron emission property is strongly related to the grain size of the cathode. The decreasing of the grain size reduces the positive charge effect of the rare earth oxide due to the electrons supplement from the metal to the rare earth oxide, whereby the secondary electrons are easier to escape into the vacuum. Y₂O₃ is introduced into Ba-W cathode to fabricate a pressed Y₂O₃-W matrix dispenser cathode. The result indicates that the secondary emission yield of the Ba-W cathode increases from 2.13 to 3.51 by adding Y₂O₃, and the thermionic emission current density (J ₀) could reach 4.18 A/cm² at 1050 °Cb.     

Solid Solution Characteristics of Pb（B1/3Nb2/3）O3-bascd Composite Ceramics

The solid solution characteristics of Pb（B1/3Nb2/3）O3-based （B=Zn^2＋, Mg^2＋, Ni^2＋） composite ceramics prepared by two-phase mixed-sintering method were developed based on dielectric measurements. Results show that there are double dielectric peaks for PZN-based composite ceramic, implying two phases coexist. However single dielectric peak was presented in PMN- and PNN-based composite ceramics, respectively. It is indicated that obvious solid solution reaction exists during the sintering process of these two systems. The effects of B-site ion difference on the solid solution characteristics were discussed by crystal chemistry. SEM was employed to investigated the microstructures of composite ceramics. The influences of solid solution reaction on grain growth were discussed.     

Microwave sintering of Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-ZrO<Subscript>2</Subscript>-WC-Co cermets

Composite powders of nanocrystalline WC-10Co (15wt%),Y2O3 (8mol%) stabilized nanocrystalline ZrO2 (30wt%),industrial cobalt powder (4.5wt%) and submicron Al2O3 (55wt%) composite powders were fabricated by high-energy ball-milling process.The nanocomposite powders were consolidated by microwave sintering process at temperature ranged 1300℃-1550℃ for 15min,respectively.The optimum consolidation conditions,such as temperature,were researched during microwave sintering process.Vickers Hardness of the consolidated cermets was measured by using a Vickers indentation test,and density of specimens was also determined by Archimedes’ principle.Microwave sintering process could not only increase the density of Al2O3-ZrO2-WC-Co cermets and reduce the porosity,but also inhibit abnormal grain growth.     

Fabrication of homogenous dispersion TiB<Subscript>2</Subscript>-Al<Subscript>2</Subscript>O<Subscript>3</Subscript> composites

In order to get a homogenous mixture and compact of TiB2-Al2O3, hybridization as a surface modification method was used to prepare nano-scale Al2O3 coated TiB2 particles. PE-wax particles were first coated onto TiB2 particles by hybridization, and then the nano-scale Al2O3 particles were coated onto the surface of TiB2 coated by PE-wax particles again. SEM, TEM and EDS were used to characterize the microstructure of as-received core/shell particles and its compacts. The experimental results show that a particle-scale homogenous dispersion of TiB2 and Al2O3 can be formed not only in mixed powder but also in dewaxed compacts. The compacts then were sintered by gas-pressing sintering (GPS). Finial products show improved mechanic properties comparing with reference samples fabricated by normal ways.     

Preparation,structure and dielectric properties of tungsten bronze ferroelectrics in SrO-Eu<Subscript>2</Subscript>O<Subscript>3</Subscript>-TiO<Subscript>2</Subscript>-Nb<Subscript>2</Subscript>O<Subscript>5</Subscript> system

Compounds Sr4Eu2Ti4Nb6O30 and Sr5EuTi3Nb7O30 with filled tetragonal tungsten bronze structure were prepared,and the dielectric characteristics and ferroelectric transition were investigated.Both ceramics displayed weak frequency dependence in room temperature dielectric constant,which decreased from 125 to 118 for Sr4Eu2Ti4Nb6O30,from 206 to 195 for Sr5EuTi3Nb7O30 in the frequency range of 10 kHz to 1 MHz.The present ceramics showed a diffuse ferroelectric phase transition.The frequency independent transition temperature (Tm) indicated the above compounds had no relaxor property.The diffuseness (γ) was 1.45 and 1.64 for Sr4Eu2Ti4Nb6O30 and Sr5EuTi3Nb7O30 respectively.The weak ferroelectric of the present materials are indicated from the P-E hysteresis loops,and a small 2Pr of 0.596 μC/cm2 and 0.068 μC/cm2 were observed for Sr4Eu2Ti4Nb6O30 and Sr5EuTi3Nb7O30 respectively.